CN106672910A - Method for preparing nano powder with strong ultraviolet absorption function - Google Patents
Method for preparing nano powder with strong ultraviolet absorption function Download PDFInfo
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- CN106672910A CN106672910A CN201710009436.0A CN201710009436A CN106672910A CN 106672910 A CN106672910 A CN 106672910A CN 201710009436 A CN201710009436 A CN 201710009436A CN 106672910 A CN106672910 A CN 106672910A
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title abstract description 16
- 238000010521 absorption reaction Methods 0.000 title abstract description 10
- 238000000889 atomisation Methods 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 17
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims abstract description 16
- 238000012986 modification Methods 0.000 claims abstract description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011787 zinc oxide Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 45
- 238000002360 preparation method Methods 0.000 claims description 38
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 235000001014 amino acid Nutrition 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000002537 cosmetic Substances 0.000 abstract description 4
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract 2
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 230000007850 degeneration Effects 0.000 abstract 1
- 238000010299 mechanically pulverizing process Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 230000000638 stimulation Effects 0.000 abstract 1
- 239000004753 textile Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 18
- 239000007789 gas Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003607 modifier Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000004137 mechanical activation Methods 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 208000035126 Facies Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Cosmetics (AREA)
Abstract
The invention provides a method for preparing nano powder with a strong ultraviolet absorption function. The method comprises the following steps: mechanically pulverizing metal oxides, and carrying out ultrasonic high-speed atomization; carrying out airflow pulverization and surface modification, thus finally obtaining a product. The zinc oxide, the cadmium oxide, the titanium dioxide and the tin dioxide used by the method for preparing the nano powder with the strong ultraviolet adsorption function have a good ultraviolet shielding function, also has the advantages of no stimulation to skin, no decomposition, no degeneration, and good thermal stability, and can be widely used in cosmetics, plastics, textiles and other industries.
Description
Technical field
The invention belongs to function nano Preparation Technique of Powders field, and in particular to a kind of strong function nano for absorbing ultraviolet
Powder preparation method.
Background technology
Ultraviolet according to wavelength can be divided into shortwave (UVC, 200-280nm), medium wave (UVB, 280-320nm), long wave (UVA,
320-400nm).Ultraviolet (UV) C is relatively unabsorbed by ozone, harm of the ultraviolet to the mankind, is typically drawn by the comprehensive function of UVA and UVB
Rise.
Nanosize metal oxide powder body less than 200nm, with good shielding ultraviolet rays function.The amount of nano-powder
Sub- dimensional effect so as to have that " widthization shows to the absorption of the light absorbs of certain wavelength with " blue-shifted phenomenon " and to various wavelength
As ", thus the absorption to ultraviolet is significantly increased.Therefore nano material is used as ultraviolet functional material is absorbed, for changing in life
Cosmetic, article of everyday use etc., with the huge market demand.
However, nano particle diameter is little, specific surface big, easily reunite, surface polarity is big, with most of polymer compatibility
Difference, is difficult to obtain dispersed on nanoscale using general blending technology；What is mixed is uneven so that existing interface changes
Property technology is difficult to the interfacial tension being completely eliminated between filler and polymeric matrix, it is difficult to realizes preferable bonding interface, does not reach
The nano-filled purpose of particle.
Additionally, both at home and abroad for prepared by metal oxide nano function powder, more using chemical technology, with high cost,
The shortcomings of complex operation, it is unfavorable for industrial applications.
The content of the invention
The purpose of this part is to summarize some aspects of embodiments of the invention and briefly introduce some preferable enforcements
Example.May do in this part and the description of the present application summary and denomination of invention a little simplified or omit to avoid making our department
Point, the purpose of specification digest and denomination of invention obscure, and this simplification or omission cannot be used for limiting the scope of the present invention.
In view of technological gap prepared by above-mentioned metal oxide nano function powder, it is proposed that the present invention.
Therefore, one of purpose of the invention is to solve deficiency of the prior art, there is provided a kind of particle diameter is little and can
The strong function nano powder preparation method for absorbing ultraviolet.
To solve above-mentioned technical problem, the invention provides following technical scheme：A kind of strong function of absorbing ultraviolet is received
Rice flour preparation, including, carry out mechanical smashing to metal-oxide, and ultrasonic high speed atomisation；Air-flow smashing is carried out, is carried out
Surface modification, finally gives product.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The ultrasonic high speed atomisation, wherein ultrasonic power are 200~250W, and high speed atomisation rotating speed is 20000~24000rpm.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The comminution by gas stream, its gas flow is 2~4m3/ min, gas pressure is 0.5~0.7MPa, and gas temperature is 90~120
℃。
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The machinery is smashed, and it smashes the time for 0.5~1h, and rotating speed is 250~350rpm.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The metal-oxide includes one or more in Zinc Oxide, Aska-Rid., titanium dioxide, tin ash.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The surface modification, wherein, the flow of dressing agent is 0.8~1.2ml/min.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The dressing agent is 1~20 μm of drop, and its mass concentration is 4~6wt.%.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The dressing agent includes the table of silane coupler series, titanate esters series or the small molecular organic compounds with 2~3 functional groups
One or more in face grafting chemical reagent.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The dressing agent includes one or more in Thioglycolic acid, amino acidses, glycerol.
As a kind of preferred version of the strong function nano powder preparation method for absorbing ultraviolet of the present invention, wherein：
The consumption of the dressing agent is the 1~10% of powder quality.
The present invention is had the advantage that：
(1) the strong function nano powder preparation method for absorbing ultraviolet provided by the present invention, using a small amount of surface modification
Agent can be prepared by the more excellent nano-powder of performance.
(2) the strong preparation-obtained nano powder of function nano powder preparation method for absorbing ultraviolet provided by the present invention
Body, particle diameter it is little and in the base have excellent surface active index and dispersibility.
(3) the strong function nano powder preparation method for absorbing ultraviolet provided by the present invention, the Zinc Oxide for being adopted, oxygen
Cadmium, titanium dioxide, tin ash, all with good shielding ultraviolet rays function, while also have it is non-stimulated to skin, regardless of
Solution, never degenerates, and the good advantage of heat stability can be widely applied to the industries such as cosmetics, plastics, weaving.
(4) the function nano powder prepared by the strong function nano powder preparation method for absorbing ultraviolet provided by the present invention
Body, after surface modification, can allow powder body dispersed in the middle of matrix, so further prepare functional material, energy
Enough give full play to the strong effect for absorbing ultraviolet.
(5) the strong function nano powder preparation method for absorbing ultraviolet provided by the present invention, with traditional chemical preparation
Method is compared, and cost is reduced, and easy to operate, the granularity of nano-powder is controllable, and production efficiency is high, can large-scale application in industrialization
Production.
Description of the drawings
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to use needed for embodiment description
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill of field, without having to pay creative labor, can be obtaining other according to these accompanying drawings
Accompanying drawing.Wherein：
Fig. 1 is the gained zinc oxide nano-powder of embodiment 1, as seen from the figure, by aoxidizing obtained in the method for the invention
Zinc nano-powder, its mean diameter is 100nm；
Fig. 2 is the gained nano TiO 2 powder of embodiment 2, as seen from the figure, by obtained in the method for the invention two
Nano titanium oxide powder, its mean diameter is 100nm；
Fig. 3 is powder body sedimentation rate test experiments result figure in embodiment 6.
Specific embodiment
It is understandable to enable the above objects, features and advantages of the present invention to become apparent from, with reference to specific embodiment pair
The specific embodiment of the present invention is described in detail.
Many details are elaborated in the following description in order to fully understand the present invention, but the present invention can be with
It is different from alternate manner described here to implement using other, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Secondly, " one embodiment " or " embodiment " referred to herein is referred to and may be included at least one realization side of the invention
Special characteristic, structure or characteristic in formula." in one embodiment " that in this manual different places occur not refers both to
Same embodiment, nor single or selectively mutually exclusive with other embodiment embodiment.
It is of the present invention to absorb ultraviolet function nano powder preparation method with strong, by combining to smashing mode, powder
Pure time, corresponding rotating speed, the advantageous embodiment for smashing the factors such as air themperature, the consumption of coating material, it is determined that final system
Preparation Method, wherein,
1st, smashing mode is combined
From in terms of cost of material, commercial metal oxide powder body does not generally reach Nano grade, or has Nano grade raw material but valency
Lattice are expensive, therefore select common grade metal-oxide powder raw material more economical；Require from feeding granularity, machinery is smashed to this simultaneously
Without strict demand, air-flow is smashed then strict demand to this, and feeding granularity crosses conference so that air-flow smashes production capacity reduction, machine damage
Consumption is big, therefore machinery smashes process coarse raw materials preferably, and air-flow smashes the fine material of process Jing machineries smashing processing preferably；
From smash powder body the distribution of powder degree, air-flow smashed compared to machinery smashing, and the particle size distribution of its output powder body is narrower；It is comprehensive
Consider that economy, machine consumption, production capacity and product standard are required, the present invention to common metal oxides powder material by carrying out
Machinery is smashed, then carries out air-flow smashing.
2nd, the smashing time that machinery is smashed
Inventor's research finds that, in the case where other conditions are constant, metal-oxide powder raw material was smashed in machinery
Cheng Zhong, if smashing overlong time, sample particle can reunite, while product cost also can be improved accordingly.
Embodiment 1
Weigh 3t Zinc Oxide coarse powder, in being added to the mechanical crusher of 350rpm rotating speeds, crush 45 minutes, and while using
Ultrasonic high speed atomisation assisted comminution, ultrasonic power is 250W, and high speed atomisation rotating speed is 24000rpm, and powder body gathers title after smashing
Weight；Coating material Thioglycolic acid 0.15t is weighed in 5wt.% ratios, air-flow disintegrating machine is adjusted, gas flow is 3m3/ min,
Gas pressure is 0.6MPa, and air themperature is 100 DEG C, and dressing agent solution concentration is 5wt.%, and the flow for modifying agent solution is
1ml/min, is atomized as 1~20 μm, start crush after spray into dressing agent, obtain after the completion of crushing average diameter for 100 nanometers,
Surface modification, finely dispersed zinc oxide nano-powder.
This is sample 1.
Embodiment 2
3t titanium dioxide coarse powder is weighed, in being added to the mechanical crusher of 300rpm rotating speeds, is crushed 60 minutes, and while adopted
With ultrasonic high speed atomisation assisted comminution, ultrasonic power is 200W, and high speed atomisation rotating speed is 22000rpm, and powder body is gathered after smashing
Weigh；Amino acidses coating material 0.24t is weighed in 8wt.% ratios, air-flow disintegrating machine is adjusted, gas flow is 3m3/
Min, gas pressure is 0.6MPa, and air themperature is 110 DEG C, and dressing agent solution concentration is 6wt.%, modifies the flow of agent solution
For 1ml/min, be atomized as 1~20 μm, start crush after spray into dressing agent, obtain after the completion of crushing average diameter for 100 nanometers,
Surface modification, finely dispersed titanium dioxide powder.
This is sample 2.
Embodiment 3
Weigh 3t Aska-Rid. coarse powder, in being added to the mechanical crusher of 250rpm rotating speeds, crush 45 minutes, and while using
Ultrasonic high speed atomisation assisted comminution, ultrasonic power is 250W, and high speed atomisation rotating speed is 20000rpm, and powder body gathers title after smashing
Weight；Glycerol 0.18t is weighed in 6wt.% ratios, air-flow disintegrating machine is adjusted, gas flow is 3m3/ min, gas pressure is
0.6MPa, air themperature is 100 DEG C, and dressing agent solution concentration is 4wt.%, and the flow for modifying agent solution is 1ml/min, is atomized
For 1~20 μm, start to spray into dressing agent after crushing, average diameter obtained after the completion of crushing for 120 nanometers, surface modification,
Finely dispersed titanium dioxide powder.
This is sample 3.
Embodiment 4
3t tin ash coarse powder is weighed, in being added to the mechanical crusher of 300rpm rotating speeds, is crushed 30 minutes, and while adopted
With ultrasonic high speed atomisation assisted comminution, ultrasonic power is 200W, and high speed atomisation rotating speed is 24000rpm, and powder body is gathered after smashing
Weigh；Glycerol 0.33t is weighed in 10wt.% ratios, air-flow disintegrating machine is adjusted, gas flow is 2m3/ min, gas pressure is
0.7MPa, air themperature be 120 DEG C, dressing agent solution concentration be 5wt.%, modify agent solution flow be 1.2ml/min, mist
Turn to 1~20 μm, start crush after spray into dressing agent, obtain after the completion of crushing average diameter for 120 nanometers, surface repair
Decorations, finely dispersed titanium dioxide powder.
This is sample 4.
Embodiment 5：
Commercially available nano level modified titanium dioxide powder is taken, its amount of modifier is 15wt%, used as sample 5.
Separately sampled product 1,2,3,4,5 each 5.0g, add 200ml deionized waters, magnetic agitation 5min to stand, and remove drift
The powder body bubbled through the water column, by the sample filtering for sinking under water, dries, weighs, and its quality is designated as M, calculates according to equation below and activates
Index：
Concrete outcome such as following table
From result, the modified powder prepared by the present invention, in terms of activation index, with excellent effect.Inventor
It has been investigated that, when amount of modifier is controlled in 1~10wt%, the activation index of modified powder can be remarkably reinforced, and stable
More than 90%.Although in commercially available modified powder, amount of modifier serious offense 10wt%, because it is in modifying process, go out
It is soft-agglomerated between existing original nano-powder and modified nano powder so as to be formed " aggregate particle size ", it is impossible to which that effectively optimization activation refers to
Number.The present invention when machinery is smashed, while with the reunion between ultrasound or high speed atomisation destruction nano-powder, it is to avoid directly add
The soft-agglomerated phenomenon for entering modifying agent and producing, and in mechanical activation comminution, simultaneously carrying out modification can corrode machine, cause mechanical disorder.
Embodiment 6：
Commercially available nano level modified titanium dioxide powder is taken, its amount of modifier is 15wt%, used as sample 5.
Separately sampled product 1,2,3,4,5, add carbon tetrachloride, are made into the dispersion liquid of 0.1wt%, and ultrasonic disperse 10min puts
In the graduated test tubes with grinding port plug of 10ml, stand at room temperature, record the solvent of the supernatant, its body with organic faciess
Product (10ml) ratio, represents the sedimentation rate of nano-powder to evaluate its dispersibility.
Timing 180 minutes, every 30 minutes sedimentation rate data, the following chart of arrangement were recorded：
From result, the modified powder prepared by the present invention, in terms of dispersibility, with excellent effect.Nano-powder
Same matrix material whether can be embodied and stablize uniformly dispersed in amalgamation and matrix material, it is critical only that control nano powder
Body uniform particle sizes and nano-powder are fully modified.Inventor's research finds, unified by mechanical activation comminution by nano-powder particle
Control using ultrasound, high speed atomisation rather than adds modifier modification in below 200nm during this, more enough to avoid modifying process
Middle modified Nano particle is soft-agglomerated with original nanoparticle, and then causes particle diameter distribution narrower, is not in that " aggregate particle size " is existing
As；Further smashed using air-flow, and while do surface modification with modifying agent, then in the case of even particle size distribution, entered
Step refining particle diameter, and while, it is modified compared to mechanical smashing method, fully nanoparticle is changed near " one-to-one "
Property.To sum up, method provided by the present invention, can control particle diameter of nanometer powder uniformly and nano-powder is fully modified, and embody
Excellent dispersibility in the base.
Embodiment 7：
Sample 1,2,3,4,5 is uniformly mixed with resin powder body PBT, wherein ultraviolet absorber is with resin-oatmeal body mass ratio
1:9；Jing twin-screw extrusions blending pelletize extrusion after mixing, extrusion temperature is 160 DEG C, and rotating speed is 150rpm, obtains uv absorption
Master batch；Master batch is put into oven drying, baking temperature is 130 DEG C, and the time is 5h；Afterwards with the uniform mixing of PET sections, wherein master batch matter
Amount accounting is 3%, and feeding spinning-drawing machine carries out melt spinning, and spinning temperature is 270 DEG C, at the beginning of speed is 600m/min, filament spinning component
Beginning pressure 8MPa, is obtained high antiultraviolet fiber；Using woven mode, antiultraviolet fiber is used in broadwise, quality accounting is
15%, obtain target fabric 1,2,3,4,5.
With Lambda35 type ultraviolet/visible light spectrogrph test fabric anti-ultraviolet (wavelength be 200~400nm) performance,
Test result is shown in Table
From result, the modified powder prepared by the present invention, in ultra-violet absorption function aspects, with excellent effect.
Function nano powder body, if can embody excellent functional effect, it is critical only that whether 1. nano-powder particles itself fully change
Property；2. whether nano-powder stably merges in the base；3. whether nano-powder is uniformly dispersed in the base.This three, it is mutually auxiliary
Coordinate.Inventor's research found, crushed by first wheel to nano-powder and simultaneously ultrasound or high velocity fog are processed, can in case
The only soft-agglomerated phenomenon of nano-powder, and then it is wide to cause it not occur particle diameter distribution because of " aggregate particle size ", it is modified not fill
Situation about dividing occurs.Consequently, it is possible in the case of the particle diameter distribution and the abundant degree that is modified of effective control nano-powder, just make
Preparation-obtained nano-powder of the invention is obtained, can have higher activation index and dispersibility excellent in the base.Enter
And, even if compared with the common commercially available function powder that modifier content is higher, the fabric prepared by the obtained powder body of the present invention,
More excellent ultraviolet radiation absorption effect can be embodied.
It is noted that chemical method is in prior art is obtained nanosize metal oxide powder body, the present invention is adopted
Physical method has made better powder body.In having abandoned traditional preparation process, the method for now modifying post processing, using ultrasound
Atomization aid in treatment, and process conditions are preferably optimized, promote " dangling bonds " that metal oxide surface atom stretches to space
Absorption to air, with the facilitation of the carrying out and ultrasonic atomizatio crushed, the three-dimensional periodic gesture inside metal-oxide
Constantly on surface by very fast interruption, electronic state and the dramatic change of body phase, cause except the stable adsorption site such as bridging oxygen room with
There are a certain degree of dissociation in gases of outer other absorption, have impact on the hybrid ionic that exists in metal-oxide system and
Covalent bond effect so that metal oxide stability dies down, can be crushed to the lower order of magnitude.
In sum, the strong function nano powder preparation method for absorbing ultraviolet provided by the present invention, using a small amount of table
Face dressing agent can be prepared by the more excellent nano-powder of performance；The strong function nano powder body for absorbing ultraviolet provided by the present invention
The preparation-obtained nano-powder of preparation method, particle diameter it is little and in the base have excellent surface active index and dispersibility；
The strong function nano powder preparation method for absorbing ultraviolet provided by the present invention, the Zinc Oxide for being adopted, Aska-Rid., titanium dioxide
Titanium, tin ash, all with good shielding ultraviolet rays function, while also not decomposing with non-stimulated to skin, never degenerate,
The good advantage of heat stability, can be widely applied to the industries such as cosmetics, plastics, weaving；It is provided by the present invention to absorb ultraviolet by force
Function nano powder body prepared by the function nano powder preparation method of line, after surface modification, can allow powder body to exist
It is dispersed in the middle of matrix, so further preparing functional material, the strong effect for absorbing ultraviolet can be given full play to；The present invention
The function nano powder preparation method of the strong absorption ultraviolet for being provided, compared with traditional chemical preparation process, cost is reduced,
Easy to operate, the granularity of nano-powder is controllable, and production efficiency is high, can large-scale application in industrialized production.
It should be noted that above example is only unrestricted to illustrate technical scheme, although with reference to preferably
Embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the technology of the present invention
Scheme is modified or equivalent, and without deviating from the spirit and scope of technical solution of the present invention, it all should cover at this
In the middle of bright right.
Claims (10)
1. it is a kind of it is strong absorb ultraviolet function nano powder preparation method, it is characterised in that：Including carrying out to metal-oxide
Machinery is smashed, and ultrasonic high speed atomisation；
Air-flow smashing is carried out, surface modification is carried out, product is finally given.
2. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 1, it is characterised in that：The ultrasound
High speed atomisation, wherein ultrasonic power are 200~250W, and high speed atomisation rotating speed is 20000~24000rpm.
3. it is according to claim 1 or claim 2 it is strong absorb ultraviolet function nano powder preparation method, it is characterised in that：It is described
Comminution by gas stream, its gas flow is 2~4m3/ min, gas pressure is 0.5~0.7MPa, and gas temperature is 90~120 DEG C.
4. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 3, it is characterised in that：The machinery
Smash, it smashes the time for 0.5~1h, rotating speed is 250~350rpm.
5. the function nano powder preparation method of ultraviolet, its feature are absorbed by force according to any one of claim 1,2 or 4
It is：The metal-oxide includes one or more in Zinc Oxide, Aska-Rid., titanium dioxide, tin ash.
6. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 5, it is characterised in that：The surface
Modification, wherein, the flow of dressing agent is 0.8~1.2ml/min.
7. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 1 or 6, it is characterised in that：It is described
Dressing agent is 1~20 μm of drop, and its mass concentration is 4~6wt.%.
8. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 7, it is characterised in that：The modification
Agent includes the surface grafting of silane coupler series, titanate esters series or the small molecular organic compounds with 2~3 functional groups
Learn one or more in reagent.
9. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 8, it is characterised in that：The modification
Agent includes one or more in Thioglycolic acid, amino acidses, glycerol.
10. the function nano powder preparation method of ultraviolet is absorbed by force according to claim 6 or 9, it is characterised in that：It is described
The consumption of dressing agent is the 1~10% of powder quality.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260366A (en) * | 2000-01-28 | 2000-07-19 | 中国科学院广州化学研究所 | Modified nm zinc oxide UV ray shielding and absorbing material |
| JP2003327430A (en) * | 2002-03-06 | 2003-11-19 | Ishihara Sangyo Kaisha Ltd | Rutile type titanium dioxide fine grain and production method thereof |
| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| CN101543466A (en) * | 2009-04-23 | 2009-09-30 | 河南大学 | Nano zinc oxide surface modifying method |
| CN103360854A (en) * | 2012-03-28 | 2013-10-23 | 厦门纳诺泰克科技有限公司 | High-transparency low-radiation energy-saving combined material for glass and preparation method thereof |
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2017
- 2017-01-06 CN CN201710009436.0A patent/CN106672910B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260366A (en) * | 2000-01-28 | 2000-07-19 | 中国科学院广州化学研究所 | Modified nm zinc oxide UV ray shielding and absorbing material |
| JP2003327430A (en) * | 2002-03-06 | 2003-11-19 | Ishihara Sangyo Kaisha Ltd | Rutile type titanium dioxide fine grain and production method thereof |
| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| CN101543466A (en) * | 2009-04-23 | 2009-09-30 | 河南大学 | Nano zinc oxide surface modifying method |
| CN103360854A (en) * | 2012-03-28 | 2013-10-23 | 厦门纳诺泰克科技有限公司 | High-transparency low-radiation energy-saving combined material for glass and preparation method thereof |
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